EP4186880A1 - Substrat métal-céramique, son procédé de fabrication et module - Google Patents

Substrat métal-céramique, son procédé de fabrication et module Download PDF

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Publication number
EP4186880A1
EP4186880A1 EP21210702.3A EP21210702A EP4186880A1 EP 4186880 A1 EP4186880 A1 EP 4186880A1 EP 21210702 A EP21210702 A EP 21210702A EP 4186880 A1 EP4186880 A1 EP 4186880A1
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EP
European Patent Office
Prior art keywords
metal
edx
layer
ceramic substrate
ceramic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP21210702.3A
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German (de)
English (en)
Inventor
Andre SCHWÖBEL
Daniel Schnee
Leszek Dr. NIEWOLAK
Miriam Dr. Rauer
Ruzica Dr. Denadic
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Heraeus Electronics & Co Kg GmbH
Original Assignee
Heraeus Deutschland GmbH and Co KG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Heraeus Deutschland GmbH and Co KG filed Critical Heraeus Deutschland GmbH and Co KG
Priority to EP21210702.3A priority Critical patent/EP4186880A1/fr
Priority to PCT/EP2022/080423 priority patent/WO2023094120A1/fr
Priority to CN202280073774.XA priority patent/CN118201894A/zh
Publication of EP4186880A1 publication Critical patent/EP4186880A1/fr
Pending legal-status Critical Current

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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
    • C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/262—Sn as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/264—Bi as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/302—Cu as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
    • B23K35/025—Pastes, creams, slurries
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    • C04B2237/127—The active component for bonding being a refractory metal
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    • C04B2237/343—Alumina or aluminates
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Definitions

  • the present invention relates to a metal-ceramic substrate, a method for producing a metal-ceramic substrate and a module having a metal-ceramic substrate.
  • Metal-ceramic substrates play an important role in the field of power electronics. They are a key element in the construction of electronic components and ensure that large amounts of heat are quickly dissipated when these components are in operation. Metal-ceramic substrates usually consist of a ceramic layer and a metal layer bonded to the ceramic layer.
  • DCB Direct Copper Bonding
  • a copper foil is provided on the surface with a copper compound (usually copper oxide) by reacting copper with a reactive gas (usually oxygen), which has a lower melting point than copper.
  • a reactive gas usually oxygen
  • the DCB method has two main disadvantages. First, the process must be carried out at relatively high temperatures, just below the melting point of copper. Second, the process can only be used for oxide-based ceramics such as alumina or superficially oxidized aluminum nitride. Therefore, there is a need for an alternative method of manufacturing metal-ceramic substrates under less stringent conditions.
  • metal foils can be bonded to ceramic bodies at temperatures of about 650 to 1000°C using a special solder containing a metal with a melting point of at least 700°C (usually silver) and an active metal.
  • the role of The active metal consists in reacting with the ceramic material and thus allowing the ceramic material to bond to the rest of the solder to form a reaction layer, while the metal with a melting point of at least 700°C serves to bond this reaction layer to the metal foil.
  • the JP4812985 B2 propose joining a copper foil to a ceramic body using a solder containing 50 to 89 percent by weight silver plus copper, bismuth and an active metal. With this method it is possible to join the copper foil to the ceramic body in a stable manner.
  • solders are based, for example, on high-melting metals (especially copper), low-melting metals (such as bismuth, indium or tin) and active metals (such as titanium).
  • high-melting metals especially copper
  • low-melting metals such as bismuth, indium or tin
  • active metals such as titanium.
  • This technology leads to a new, independent class of connection, since the basis of the solder used is formed by a different metal (copper instead of silver), which leads to changed material properties and an adjustment with regard to the other solder components and modified joining conditions .
  • the metal-ceramic substrates produced in this way therefore have, in addition to a metal layer and a ceramic body, a connecting layer which lies between the metal layer and the ceramic body and contains an active metal.
  • the object of the present invention is therefore to provide a metal-ceramic substrate which, on the one hand, has a connection between the metal layer and the ceramic body with high stability and, on the other hand, has high thermal and electrical conductivity.
  • a further object of the present invention is therefore to provide such a metal-ceramic substrate which does not have the problems which occur in connection with silver migration.
  • the invention provides a method for producing a metal-ceramic substrate and a module having a metal-ceramic substrate.
  • the metal-ceramic substrate according to the invention comprises a ceramic body, a metal layer and a connection layer.
  • the connecting layer is located between the ceramic body and the metal layer in the metal-ceramic substrate.
  • the connecting layer is therefore preferably in contact with the ceramic body and the metal layer.
  • the metal-ceramic substrate contains a ceramic body, a (first) metal layer, a (first) connection layer which is in contact with the ceramic body and the first metal layer, a second metal layer and a second connection layer which is in contact with the ceramic body and the second metal layer is in contact.
  • the composition of the first connection layer preferably corresponds to the composition of the second connection layer.
  • the ceramic body preferably has a first surface and a second surface.
  • the metal layer preferably has a first surface. If present, the second metal layer preferably has a first surface.
  • the (first) connecting layer is located in the metal-ceramic substrate between the first surface of the ceramic body and the first surface of the (first) metal layer.
  • the metal-ceramic substrate contains a second connection layer which is in contact with the second surface of the ceramic body and the first surface of the second metal layer.
  • the (first) connection layer is preferably located in the metal-ceramic substrate between the first surface of the ceramic body and the first surface of the (first) metal layer and the second connection layer is located between the second surface of the ceramic body and the first surface of the second metal layer.
  • the ceramic of the ceramic body is preferably an insulating ceramic.
  • the ceramic is selected from the group consisting of oxide ceramics, nitride ceramics and carbide ceramics.
  • the ceramic is selected from the group consisting of metal oxide ceramics, silicon oxide ceramics, metal nitride ceramics, silicon nitride ceramics, boron nitride ceramics and boron carbide ceramics.
  • the ceramic is selected from the group consisting of aluminum nitride ceramics, silicon nitride ceramics and aluminum oxide ceramics (such as ZTA ("Zirconia Toughened Alumina") ceramics).
  • the ceramic body consists of (1) at least one element selected from the group consisting of silicon and aluminum, (2) at least one element selected from the group consisting of oxygen and nitrogen, optionally (3) at least one element selected from the group consisting of (3a) rare earth metals, (3b) metals of the second main group of the periodic table of elements, (3c) zirconium, (3d) copper, (3e) molybdenum and (3f) silicon, and optionally (4) unavoidable impurities.
  • the ceramic body is free from bismuth, gallium and zinc.
  • the ceramic body preferably has a thickness of 0.05-10 mm, more preferably in the range of 0.1-5 mm and particularly preferably in the range of 0.15-3 mm.
  • the metal of the metal layer is preferably selected from the group consisting of copper, aluminum and molybdenum. According to a particularly preferred embodiment, the metal of the metal layer is selected from the group consisting of copper and molybdenum. According to a very particularly preferred embodiment, the metal of the metal layer is copper. According to another very particularly preferred embodiment, the metal layer consists of copper and unavoidable impurities.
  • the metal layer preferably has a thickness in the range of 0.01-10 mm, particularly preferably in the range of 0.03-5 mm and very particularly preferably in the range of 0.05-3 mm.
  • the connecting layer comprises (i) a metal M1 with a melting point of at least 700°C, (ii) a metal M2 with a melting point of less than 700°C, (iii) a metal M3 selected from the group of active metals, and (iv) a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium.
  • connection layer is preferably understood to mean the area of the metal-ceramic substrate that is located between the ceramic body and the metal layer.
  • the bonding layer comprises (i) a metal M1 having a melting point of at least 700°C.
  • the metal M1 with a melting point of at least 700°C preferably has a melting point of at least 850°C and more preferably has a melting point of at least 1000°C.
  • the metal M1 having a melting point of at least 700°C is selected from the group consisting of copper, nickel, tungsten and molybdenum.
  • the metal M1 having a melting point of at least 700°C is copper.
  • the bonding layer comprises (ii) a metal M2 having a melting point of less than 700°C.
  • the metal M2 having a melting point of less than 700°C preferably has a melting point of less than 600°C and more preferably has a melting point of less than 550°C. According to a particularly preferred embodiment, the metal M2 having a melting point of less than 700°C is tin.
  • the connecting layer comprises (iii) a metal M3 selected from the group of active metals.
  • the metal M3 is therefore preferably a metal which creates a connection to the ceramic by chemical reaction.
  • the metal M3 is selected from the group consisting of hafnium, titanium, zirconium, niobium, cerium, tantalum and vanadium.
  • the metal M3 is selected from the group consisting of hafnium, titanium, zirconium, niobium and cerium.
  • the metal M3 is selected from the group consisting of hafnium, titanium and zirconium.
  • the metal M3 is titanium.
  • the connection layer comprises (iv) a metal M4.
  • the metal M4 is a metal selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium. According to a particularly preferred embodiment, the metal M4 is selected from the group consisting of bismuth, gallium and zinc. According to a most preferred embodiment, the metal M4 is bismuth.
  • the metals M1, M2, M3 and M4 are different metals.
  • the bonding layer which is between the ceramic body and the metal layer, therefore comprises each of the metals M1, M2, M3 and M4.
  • the connecting layer that is between the ceramic body and the metal layer (i) a metal M1 with a melting point of at least 700°C, (ii) a metal M2 with a melting point of less than 700°C, (iii) a metal M3 selected from the group of active metals, and (iv) a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, the metals M1, M2, M3 and M4 being different.
  • the metal M2 having a melting point less than 700°C is not selected from the group consisting of bismuth, gallium, zinc, indium, aluminum and magnesium. Furthermore, the metal M2 is not an active metal. Likewise, the metal M1 having a melting point of at least 700°C is not germanium. In addition, the metal M1 having a melting point of at least 700°C is not an active metal.
  • a metal-ceramic substrate provided that on the one hand has a particularly stable connection between the ceramic body and the metal layer and on the other hand a high electrical and thermal conductivity.
  • the silver content in the connecting layer, determined by EDX is not more than 10 percent by weight. Accordingly, the invention also includes embodiments in which the connecting layer is silver-free, ie the silver content in the connecting layer determined by means of EDX is 0 percent by weight.
  • the absence of silver or the presence of only small amounts of silver can prevent or reduce unwanted migration of silver at the edges of the connecting layer in the metal-ceramic substrate.
  • the content of metal M1 in the connecting layer (M(M1) EDX ) determined by means of EDX is in the range of 65-89 percent by weight. According to a particularly preferred embodiment, the content of metal M1 in the connecting layer (M(M1) EDX ) determined by means of EDX is in the range of 67-88 percent by weight. According to a very particularly preferred embodiment, the content of metal M1 in the connecting layer (M(M1) EDX ) determined by means of EDX is in the range of 70-88 percent by weight.
  • the content of metal M3 in the connecting layer (M(M3) EDX ) determined by means of EDX is in the range of 0.5-15 percent by weight. According to a particularly preferred embodiment, the content of metal M3 in the connecting layer (M(M3) EDX ) determined by means of EDX is in the range of 0.5-14 percent by weight. According to a very particularly preferred embodiment, the content of metal M3 in the connecting layer (M(M3) EDX ) determined by means of EDX is in the range from 1-14 percent by weight.
  • the content of metal M4 in the connecting layer (M(M4) ICP ) determined by ICP is in the range of 0.01-2% by weight. According to a particularly preferred embodiment, the content of metal M4 in the connecting layer (M(M4) ICP ) determined by ICP is in the range of 0.01-1.5 percent by weight. According to a very particularly preferred embodiment, the content of metal M4 in the connecting layer (M(M4) ICP ), determined by means of ICP, is in the range of 0.1-1 percent by weight.
  • the metal-ceramic substrate according to the invention can be produced in a manner customary in the art.
  • a stack is first provided that includes a ceramic body, a metal foil, and a brazing material in contact with the ceramic body and the metal foil.
  • the brazing material is preferably located between the ceramic body and the metal foil.
  • the stack includes a ceramic body, a (first) metal foil, a (first) braze material that is in contact with the ceramic body and the first metal foil, a second metal foil, and a second braze material that is in contact with the ceramic body and the second metal foil is in contact.
  • a (first) soldering material is preferably located between the ceramic body and the (first) metal foil and a second soldering material is located between the ceramic body and the second metal foil.
  • the first brazing material preferably corresponds to the second brazing material.
  • the ceramic body, the metal foil and the soldering material are preferably designed in such a way that the metal-ceramic substrate according to the invention is formed after heating.
  • the ceramic body and the metal foil are preferably configured as described above in relation to the ceramic body and the metal layer of the metal-ceramic substrate.
  • the brazing material preferably comprises (i) a metal M1 having a melting point of at least 700°C, (ii) a metal M2 having a melting point less than 700°C, (iii) a metal M3 selected from the group of active metals , and (iv) a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium.
  • the metal M1, the metal M2, the Metal M3 and the metal M4 are preferably configured as described above in relation to the connection layer of the metal-ceramic substrate.
  • the brazing material in contact with the ceramic body and the metal foil comprises each of the metals M1, M2, M3 and M4. Accordingly, the brazing material in contact with the ceramic body and the metal foil comprises (i) a metal M1 having a melting point of at least 700°C, (ii) a metal M2 having a melting point less than 700°C, (iii) a metal M3 selected from the group of active metals, and (iv) a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, the metals M1, M2, M3 and M4 are different.
  • the metal M2 having a melting point less than 700°C is not selected from the group consisting of bismuth, gallium, zinc, indium, aluminum and magnesium. Furthermore, the metal M2 is not an active metal. Likewise, the metal M1 having a melting point of at least 700°C is not germanium. In addition, the metal M1 having a melting point of at least 700°C is not an active metal.
  • the solder material preferably comprises at least one metal component comprising (i) metal M1, (ii) metal M2, (iii) metal M3, and (iv) metal M4.
  • the brazing material comprises: a metal component (i) containing the metal M1, a metal component (ii) containing the metal M2, a metal component (iii) containing the metal M3, and a Metal component (iv) containing the metal M4.
  • the brazing material comprises: a metal component (i) containing a member selected from the group consisting of (i) a metal M1, (ii) a metal M2, (iii) a metal M3 and ( iv) a metal M4, and at least one further metal component (ii) selected from the group consisting of (i) a metal M1, (ii) a metal M2, (iii) a metal M3 and (iv) a metal M4 consists, contains, which are not contained in metal component (i).
  • the concept of the metal component is not further restricted.
  • metals and metal alloys it also includes metal compounds such as intermetallic phases and other compounds (such as e.g. metal hydrides). According to a preferred embodiment, the metal component is therefore selected from the group consisting of metals, metal alloys and metal compounds.
  • the brazing material preferably comprises (i) a metal M1 having a melting point of at least 700°C.
  • the brazing material comprises a metal component (i) containing a metal M1 with a melting point of at least 700°C.
  • the soldering material comprises a metal component (i) containing copper.
  • metal component (i) is copper.
  • the brazing material preferably comprises (ii) a metal M2 having a melting point of less than 700°C.
  • the brazing material comprises a metal component (ii) containing a metal M2 with a melting point of less than 700°C.
  • the metal component (ii) is an alloy of a metal M2 with a melting point of less than 700° C. with another metal.
  • the other metal can be selected, for example, from the group consisting of metals M1 with a melting point of less than 700 ° C, metals M2 with a melting point of at least 700 ° C, metals M3, which are selected from the group of active metals, and metals M4 selected from the group consisting of bismuth, indium, germanium, gallium and zinc.
  • the metal component (ii) containing a metal M2 with a melting point of less than 700° C. is selected from the group consisting of tin, tin-copper alloys, tin-bismuth alloys, tin-antimony alloys , tin-zinc-bismuth alloys and indium-tin alloys.
  • the brazing material preferably comprises a metal M3 selected from the group of active metals.
  • the soldering material comprises a metal component (iii) containing a metal M3 selected from the group of active metals.
  • the metal component (iii) is an active metal alloy or an active metal compound, particularly preferably an active metal hydride.
  • the Metal component (iii) is preferably selected from the group consisting of titanium hydride, titanium-zirconium-copper alloys, zirconium hydride and hafnium hydride.
  • the metal component (iii) is selected from the group consisting of hafnium hydride, titanium hydride and zirconium hydride.
  • the metal component (iii) is titanium hydride.
  • the brazing material preferably comprises an M4 metal.
  • the brazing material comprises a metal component (iv) containing a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium.
  • the brazing material comprises a metal component (iv) containing bismuth.
  • metal component (iv) is bismuth.
  • the proportion of the metal M1 with a melting point of at least 700° C. is 65-89 percent by weight, more preferably 67-88 percent by weight and most preferably 70-88 percent by weight, based on the total metal weight of the brazing material.
  • the proportion of the metal M2 with a melting point of less than 700° C. is 10-20% by weight, particularly preferably 10-18% by weight and very particularly preferably 10-15% by weight, based on the total metal weight of the brazing material.
  • the proportion of the metal M3 selected from the group of active metals is 0.5-15 percent by weight, more preferably 0.5-14 percent by weight and most preferably 1-14 percent by weight, based on the total metal weight of the soldering material.
  • the proportion of the metal M4, which is selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium is 0.01-2 percent by weight, particularly preferably 0.01-1 .5% by weight and most preferably 0.1-1% by weight based on the total metal weight of the braze material.
  • the solder material is preferably silver-free or low-silver. Therefore, the proportion of silver is preferably less than 10 percent by weight, more preferably less than 5 percent by weight and most preferably less than 1 percent by weight based on the total metal weight of the braze material.
  • the brazing material is in contact with the ceramic body and the metal foil. Accordingly, the brazing material is preferably located between the ceramic body and the metal foil.
  • the brazing material can be provided on the ceramic body and then the metal foil can be applied to the brazing material.
  • the brazing material is preferably at least one material selected from the group consisting of pastes, foils and deposits containing a metal M1 with a melting point of at least 700°C, a metal M2 with a melting point of less than 700°C, a metal M3 selected from the group of active metals and a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium.
  • the soldering material can be a paste.
  • the paste preferably contains (a) at least one metal component, which is a metal M1 with a melting point of at least 700° C., a metal M2 with a melting point of less than 700° C., a metal M3 selected from the group of active metals, and a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, and (b) an organic medium.
  • the organic medium is preferably an organic medium commonly used in the technical field concerned.
  • the organic medium contains an organic binder, an organic dispersant, or a mixture thereof.
  • the organic binder is preferably removed from the solder material upon heating.
  • the organic binder is preferably a thermoplastic or duroplastic.
  • organic binders include cellulose derivatives (such as ethyl cellulose, butyl cellulose, and cellulose acetate), polyethers (such as polyoxymethylene), and acrylic resins (such as polymethyl methacrylate and polybutylene methacrylate).
  • the organic dispersing agent is preferably an organic compound which gives the paste an appropriate viscosity and which is expelled when the paste is dried or heated.
  • the organic dispersant may be selected from, for example, aliphatic alcohols, terpene alcohols, alicyclic alcohols, aromatic cyclic carboxylic acid esters, aliphatic esters, carbitols and aliphatic polyols.
  • organic dispersant examples include octanol, decanol, terpineols (eg, dihydroterpineol), cyclohexanol, dibutyl phthalate, carbitol, ethyl carbitol, ethylene glycol, butanediol, and glycerin.
  • the paste can also contain customary additives.
  • additives include inorganic binders (such as glass frits), stabilizers, surfactants, dispersants, rheology modifiers, wetting aids, defoamers, fillers, and hardeners.
  • the proportion of the at least one metal component is a metal M1 with a melting point of at least 700° C., a metal M2 with a melting point of less than 700° C., a metal M3 selected from the group of active metals and a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, 20-95% by weight, more preferably 30-95% by weight and most preferably 75-95% Percentage by weight based on the total weight of the paste.
  • the proportion of the organic medium is 5-80% by weight, more preferably 5-70% by weight and particularly preferably 5-25% by weight, based on the total weight of the paste.
  • the ratio of the total weight of (a) at least one metal component, which is a metal M1 having a melting point of at least 700° C., a metal M2 having a melting point of less than 700° C., a metal M3 consisting of is selected from the group of active metals and a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium by weight of (b) organic medium at least 5:1 , more preferably at least 7:1 and most preferably at least 8: 1.
  • the ratio of the total weight of (a) at least one metal component which is a metal M1 having a melting point of at least 700 ° C, a metal M2 having a melting point of less than 700 °C, a metal M3 selected from the group of active metals and a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, for the weight of (b) organic medium in the range from 1:1 to 20:1, more preferably in the range from 2:1 to 20:1 and most preferably in the range from 5:1 to 15:1.
  • the paste is preferably applied to the surface of the ceramic body.
  • the paste can be applied by a dispersing method or a printing method, for example. Suitable printing methods are, for example, screen printing methods, inkjet printing methods and offset printing methods.
  • the paste is applied to the surface of the ceramic body by a screen printing process.
  • the paste After applying the paste, the paste can be pre-dried if necessary.
  • the pre-drying can take place at room temperature or at elevated temperature. Pre-drying conditions may vary depending on the organic medium contained in the paste.
  • the pre-drying temperature can be, for example, in the range of 50-180°C and is preferably in the range of 80-150°C.
  • the pre-drying usually takes place for a period of 2 minutes to 2 hours and preferably for a period of 5 minutes to 1 hour.
  • the surface of the metal foil can then be applied to the paste, which has been pre-dried if necessary, in order to obtain a stack.
  • the soldering material can also be a foil.
  • the foil comprises a metal M1 having a melting point of at least 700°C, a metal M2 having a melting point less than 700°C, a metal M3 selected from the group of active metals, and a metal M4 selected from the group is selected from bismuth, gallium, zinc, indium, germanium, aluminum and magnesium exists.
  • the film can include other components, such as a suitable binder.
  • the foil can be obtained, for example, by using at least one metal component which is a metal M1 with a melting point of at least 700°C, a metal M2 with a melting point of less than 700°C, a metal M3 selected from the group of active metals and a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, and optionally other components are homogenized and heated to a temperature below the melting point of the metal M1 with a melting point of at least 700°C, metal M2 with a melting point of less than 700°C, active metal M3 and metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium , aluminum and magnesium, but which is sufficient to form a bond between the metals.
  • This temperature can be at least 200°C, for example.
  • the foil can be obtained, for example, by using at least one metal component that is a metal M1 with a melting point of at least 700°C, a metal M2 with a melting point of less than 700°C, a metal M3 that is from the group of active metals and a metal M4 selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, and a binder are mixed and the mixture is formed into a green body and heated. When heated, the binder can harden and form a matrix in which the metals are distributed.
  • the film can be placed on the ceramic, for example.
  • the surface of the metal foil can then be applied to the foil on the ceramic in order to obtain a stack.
  • the brazing material may be a deposit.
  • the soldering material can be deposited, for example, by electrolytic deposition or vapor deposition.
  • the soldering material is deposited on the ceramic body. After that you can the metal foil can be applied to the solder material deposited on the ceramic to obtain a stack.
  • the stack is heated to obtain a metal-ceramic substrate.
  • the heating takes place in order to obtain a metal-ceramic substrate with the formation of a material connection between the ceramic body and the metal foil via the soldering material.
  • the material connection is preferably formed by the metal M3 entering into a connection with the ceramic body during heating and the metal M1 with a melting point of at least 700° C., the metal M2 with a melting point of less than 700° C., the metal M4, selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium and the metal of the metal foil combine to form an alloy.
  • a material connection is then formed between the ceramic body and the metal foil via the active metal M3 connected to the ceramic body and the resulting alloy.
  • the stack When heated, the stack is heated to a peak temperature.
  • the peak temperature is not further limited and is preferably equal to or less than the melting point of the metal M1 having a melting point of at least 700°C and lower than the melting point of the metal of the metal foil.
  • the peak temperature is at least 10°C and more preferably at least 50°C below the melting point of the metal of the metal foil.
  • the peak temperature is at least 700°C.
  • the peak temperature is preferably in the range of 700-1100°C, more preferably in the range of 750-1050°C, and most preferably in the range of 800-1000°C.
  • peak temperature refers to the temperature measured at the stack using a thermocouple.
  • the peak temperature is the maximum temperature measured on the stack. In order to prevent adverse effects such as excessive contraction or oozing of the molten metal due to excessive molten metal fluidity, those skilled in the art will endeavor to avoid excessively high peak temperatures.
  • the high-temperature heating time herein preferably refers to the length of time that the stack is heated to a temperature at least equal to the peak temperature - 250°C. Therefore, with an exemplary peak temperature of 900°C, the high temperature heating time corresponds to the length of time that the stack is exposed to at least a temperature of 650°C during heating.
  • the high-temperature heating time is no more than 60 minutes, more preferably no more than 50 minutes, particularly preferably no more than 45 minutes and very particularly preferably no more than 40 minutes.
  • the high-temperature heating time is preferably in the range of 2-60 minutes, more preferably in the range of 3-50 minutes, particularly preferably in the range of 5-45 minutes and most preferably in the range of 10-40 minutes.
  • the stack is preferably heated in that, starting from a heating zone, the energy required for heating is introduced in the direction of the stack.
  • the material connection is preferably formed by the metal M3 entering into a connection with the ceramic body and the metal M1 with a melting point of at least 700° C., the metal M2 with a melting point of less than 700° C., the metal M4, which consists of is selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, and the metal of the metal foil combine to form an alloy.
  • the metal M4 which consists of is selected from the group consisting of bismuth, gallium, zinc, indium, germanium, aluminum and magnesium, and the metal of the metal foil combine to form an alloy.
  • a material bond is then formed between the ceramic body and the metal foil via the active metal M3, which is connected to the ceramic body, and the alloy.
  • the stack is heated in a furnace, preferably in a continuous furnace or in a chamber furnace.
  • a non-oxidizing atmosphere is preferably present in the heating zone.
  • the non-oxidizing atmosphere is preferably an inert gas atmosphere.
  • a nitrogen atmosphere, a helium atmosphere or an argon atmosphere is preferably present in the heating zone.
  • a nitrogen atmosphere is present in the heating zone.
  • the proportion of a reactive gas, in particular oxygen, in the non-oxidizing atmosphere is less than 1000 ppm, more preferably less than 500 ppm and particularly preferably less than 40 ppm.
  • a material connection is preferably formed between the ceramic body and the metal foil via the soldering material, with the result that a metal-ceramic substrate is obtained, which has a ceramic body, a metal layer and a connecting layer located between the ceramic body and the metal layer .
  • the metal-ceramic substrate can be subjected to further treatment steps.
  • the metal-ceramic substrate preferably the exposed surface of the metal layer of the metal-ceramic substrate, can be polished.
  • the metal layer surface of the metal-ceramic substrate is polished physically or chemically.
  • the metal-ceramic substrate can be structured.
  • the metal-ceramic substrate can be provided with conductor tracks. The conductor tracks are preferably produced by etching.
  • the metal-ceramic substrate according to the invention can be used in particular for applications in electronics, especially in the field of power electronics.
  • the invention therefore also provides a module that has a metal-ceramic substrate as described above.
  • such a module includes a base plate. This base plate is preferably connected areally to the metal layer of the metal-ceramic substrate.
  • the module comprises at least one chip. The at least one chip is preferably connected areally to the metal layer of the at least one metal-ceramic substrate.
  • the module comprises a metal-ceramic substrate having a first metal layer and a second metal layer (the first metal layer preferably being opposite the second metal layer), a base plate and at least one chip, the at least one chip having the first metal layer of the metal-ceramic substrate and the bottom plate is connected to the second metal layer of the metal-ceramic substrate.
  • the content of the metals M1, M2, M3 and silver in the connecting layer is preferably determined as follows:
  • the metal-ceramic substrate to be examined is first cut perpendicular to a plane spanned by the metal layer of the metal-ceramic substrate by sawing with a diamond saw blade at low speed and using an oil-based lubricant (Buehler).
  • a cuboid sample blank with a rectangular base area in the range from 100 mm 2 to 400 mm 2 was cut out. Accordingly, the sample blank has a sample surface that is subjected to the examination. This sample surface therefore runs perpendicular to the plane spanned by the metal layer of the metal-ceramic substrate before sawing.
  • the sample blank is first embedded in a mold with a low-shrinkage epoxy resin (Epo-Fix, Struers), with the sample surface oriented perpendicular to the mold wall.
  • Epo-Fix, Struers low-shrinkage epoxy resin
  • the epoxy resin is then cured at room temperature.
  • the sample surface of the sample blank is mechanically polished with an automated polishing device (Tegrapol, Struers) to achieve a roughness of 1 ⁇ m or less.
  • the polished sample surface is conductively coated with iridium to a thickness of 1-5 nm using a metal sputtering device (Q150T, Quorum Technologies).
  • an analysis zone on the sample surface is examined using scanning electron microscopy - energy dispersive X-ray spectroscopy (SEM-EDX).
  • SEM-EDX scanning electron microscopy - energy dispersive X-ray spectroscopy
  • a focused primary electron beam is scanned point by point over the sample surface.
  • the scattered electrons are recorded with a detector, whereby the number of electrons per pixel results in a microscopic image of the sample surface in shades of gray.
  • the primary electron beam stimulates the sample to emit characteristic X-rays, whereby the elements in the sample and their proportion by weight can be determined by analyzing the energy spectrum with an EDX detector.
  • a scanning electron microscope JSM-6060 SEM, JEOL Ltd
  • a silicon drift EDX detector NORAN, Thermo Scientific Inc
  • analysis software Paneer Mountaineer EDS System, for example version 2.8, Thermo Scientific Inc
  • the spectrum is analyzed.
  • the elements to be examined are selected and the elements contained in the ceramic body (the presence of which can optionally be determined in advance by a conventional examination method), iridium and elements of the epoxy resin are deselected.
  • the amount of each of the elements to be tested is given in weight percent, with the total being 100%.
  • the third to sixth steps are repeated nine times at different points.
  • the mean value is then determined from the values obtained from a total of ten individual measurements.
  • the ratio [M(M4)/M(M2)] ICP in the connection layer of the metal-ceramic substrate is preferably determined as follows:
  • the sample solution thus obtained is transferred to a tared polyethylene bottle.
  • the sample solution is then diluted with water according to an expected value in relation to the content of the element to be examined.
  • An aliquot of the sample solution is transferred to a 100 ml volumetric flask containing 10 ml hydrochloric acid (30% by weight), 10 ml saline buffer (10 g/l sodium chloride) and a calibration standard (e.g. a 1 g/l yttrium solution).
  • the measurement solution obtained in this way is measured by ICP-OES (optical emission spectrometry; inductively coupled plasma—optical emission spectrometry) with regard to the [M(M4)/M(M2)] ICP ratio against the calibration standard.
  • the ICP emission spectrometer iCAP 6500 Duo (Thermo Scientific Inc) is used for this, with the following plasma settings being made for the measurement: purge pump rate (rpm): 35; Analysis pump rate (rpm): 35; Pump hose type: Tygon Orange/white; RF Power: 1150W; Nebulizer gas: 0.60 l/min; Auxiliary gas: 0.5 l/min.
  • the present invention is illustrated by the following non-limiting examples of embodiment.
  • metal-ceramic substrates (Examples 1 - 8 and Comparative Examples 1 - 7): In Examples 1 - 8 and Comparative Examples 1 - 7, metal-ceramic substrates differing in the composition of the bonding layer were prepared. In each case, a stack containing a ceramic body, a metal foil and a soldering material that is in contact with the ceramic body and the metal foil was provided and then heated. The metal-ceramic substrates obtained in this way were then tested with regard to their bond strength and their thermal and electrical conductivity.
  • tin, titanium hydride and bismuth as a powder in the specified amounts were successively introduced into the specified amount of the organic vehicle containing Texanol and mixed at 35 Hz for 20 minutes in a stand mixer until a homogeneous paste was obtained in each case. Thereafter, the copper powder was added in increments. The mixture thus produced was stirred until a homogeneous paste was obtained.
  • ceramic bodies were bonded to copper foils on both sides of their opposite surfaces.
  • ceramic bodies with the dimensions 177.8 ⁇ 139.7 ⁇ 0.32 mm (obtained from Toshiba Materials) were used, which had identical front and rear surfaces.
  • the respective paste was screen-printed using a 165-mesh screen over an area measuring 137 ⁇ 175 mm 2 on the back of such a ceramic body and pre-dried at 125° C. for 15 minutes.
  • the paste thickness after pre-drying was 35 +/- 5 ⁇ m. Thereafter, the arrangement produced in this way was turned over, the paste was printed in the same way on the front side of the ceramic body and pre-dried.
  • the ceramic provided with paste on both sides was provided with copper foil made of oxygen-free, highly conductive copper with a purity of 99.99% and dimensions of 174 x 137 x 0.3 mm on both sides in order to obtain a stack with the following structure: copper foil - pre-dried paste - Ceramic - pre-dried paste - copper foil.
  • the stack was then heated in a continuous furnace.
  • a silicon carbide plate was first placed on the transport chain of a continuous furnace, to which a graphite foil was applied.
  • the structure was then transported on the transport chain through the heating zone of a continuous furnace and within 25 minutes from 50°C to a peak temperature of 935°C (measured with a type K thermocouple from the company Temperatur Messmaschine Hettstedt GmbH on the stack) for 2 minutes heated.
  • the temperature of the assembly was then cooled back down to 50°C within 25 minutes.
  • the metal-ceramic substrates thus obtained were then cooled to room temperature to obtain metal-ceramic substrates each including a ceramic layer bonded on both sides to a copper layer via a bonding layer.
  • M(M2) EDX Content [in percent by weight] of tin (metal M2) in the connecting layer determined by means of EDX.
  • M(Ag) EDX Content [in percent by weight] of silver in the connecting layer determined by means of EDX.
  • connection layer cumulatively in relation to the connection layer, have a stable connection between the metal layer and the ceramic body with high thermal and electrical conductivity at the same time.
  • these metal-ceramic substrates are silver-free, the problems associated with silver migration do not arise.
  • the connection between the metal layer and the ceramic body is less stable in comparison, or the metal-ceramic substrates obtained have low thermal and electrical conductivity .

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  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
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EP21210702.3A 2021-11-26 2021-11-26 Substrat métal-céramique, son procédé de fabrication et module Pending EP4186880A1 (fr)

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EP21210702.3A EP4186880A1 (fr) 2021-11-26 2021-11-26 Substrat métal-céramique, son procédé de fabrication et module
PCT/EP2022/080423 WO2023094120A1 (fr) 2021-11-26 2022-11-01 Substrat métallo-céramique, son procédé de production, et module
CN202280073774.XA CN118201894A (zh) 2021-11-26 2022-11-01 金属-陶瓷基板、其生产方法以及模块

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Citations (11)

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JPS4812985B1 (fr) 1967-03-15 1973-04-24
US3744120A (en) 1972-04-20 1973-07-10 Gen Electric Direct bonding of metals with a metal-gas eutectic
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GB1357073A (en) * 1972-08-02 1974-06-19 Asahi Glass Co Ltd Process for soldering difficultly-solderable material having oxide surface
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DE2308041A1 (de) * 1972-02-19 1973-08-23 Asahi Glass Co Ltd Lotlegierung und verwendung derselben
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DE2319854C2 (de) 1972-04-20 1983-12-29 General Electric Co., Schenectady, N.Y. Verfahren zum direkten Verbinden eines Metallteiles mit einem aus nichtmetallischem Material bestehenden Substraten
US3949118A (en) * 1972-07-21 1976-04-06 Asahi Glass Company, Ltd. Process for soldering difficultly solderable material having oxide surface and a solder alloy therefor
GB1357073A (en) * 1972-08-02 1974-06-19 Asahi Glass Co Ltd Process for soldering difficultly-solderable material having oxide surface
SU631288A1 (ru) * 1977-06-10 1978-11-05 Всесоюзный Научно-Исследовательский Инструментальный Институт Припой дл пайки инструментальных материалов
US4603090A (en) * 1984-04-05 1986-07-29 Gte Products Corporation Ductile titanium-indium-copper brazing alloy
US5906897A (en) * 1996-01-26 1999-05-25 Ngk Spark Plug Co., Ltd. Al metal joined body
DE102017114893A1 (de) 2017-07-04 2019-01-10 Rogers Germany Gmbh Lötmaterial zum Aktivlöten und Verfahren zum Aktivlöten
CN113528884A (zh) * 2021-07-21 2021-10-22 广东省科学院中乌焊接研究所 铜基中间层合金及其制备方法、陶瓷和无氧铜的复合连接件及其焊接方法

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